Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email CHRISTOU@CHEM.UFL.EDU _publ_contact_author_name 'Prof George Christou' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry University of Florida PO Box 117200 Gainesville FL 32611-7200 UNITED STATES OF AMERICA ; _publ_section_title ; Preparation and properties of new Fe6 and Fe8 Clusters of iron(III) with tripodal ligands ; loop_ _publ_author_name 'George Christou' 'Khalil Abboud' 'Muralee Murugesu' data_xm41 _database_code_CSD 217872 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H99 Fe8 N5 O33' _chemical_formula_weight 2213.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.1207(10) _cell_length_b 27.2142(14) _cell_length_c 19.3376(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.881(2) _cell_angle_gamma 90.00 _cell_volume 9172.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 130 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4560 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7290 _exptl_absorpt_correction_T_max 0.9039 _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 80936 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.50 _reflns_number_total 20947 _reflns_number_gt 16785 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+10.0305P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000030(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 20947 _refine_ls_number_parameters 1220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.72258(2) -0.738845(16) 0.16456(2) 0.02417(10) Uani 1 1 d . . . Fe2 Fe 0.61487(2) -0.668854(16) 0.20618(2) 0.02217(10) Uani 1 1 d . . . Fe3 Fe 0.73064(2) -0.676266(16) 0.34374(2) 0.02337(10) Uani 1 1 d . . . Fe4 Fe 0.66565(3) -0.783192(16) 0.31816(2) 0.02551(10) Uani 1 1 d . . . Fe5 Fe 0.51448(2) -0.709801(16) 0.29037(2) 0.02477(10) Uani 1 1 d . . . Fe6 Fe 0.61108(2) -0.599827(16) 0.37007(2) 0.02246(10) Uani 1 1 d . . . Fe7 Fe 0.66372(2) -0.564134(16) 0.22350(2) 0.02201(10) Uani 1 1 d . . . Fe8 Fe 0.82569(2) -0.642204(16) 0.23892(2) 0.02216(10) Uani 1 1 d . . . O1 O 0.69865(13) -0.79134(8) 0.22836(11) 0.0294(5) Uani 1 1 d . . . O2 O 0.74872(12) -0.70400(8) 0.07884(11) 0.0304(5) Uani 1 1 d . . . O3 O 0.61684(11) -0.71355(8) 0.12864(11) 0.0270(5) Uani 1 1 d . . . O4 O 0.73270(11) -0.68317(7) 0.22897(10) 0.0224(4) Uani 1 1 d . . . O5 O 0.82930(12) -0.76530(8) 0.18820(12) 0.0323(5) Uani 1 1 d . . . O6 O 0.60623(12) -0.60981(7) 0.14823(10) 0.0258(5) Uani 1 1 d . . . O7 O 0.50552(11) -0.67712(8) 0.19660(11) 0.0267(5) Uani 1 1 d . . . O8 O 0.62137(11) -0.71678(7) 0.29045(11) 0.0231(4) Uani 1 1 d . . . O9 O 0.65057(11) -0.61795(7) 0.28578(10) 0.0220(4) Uani 1 1 d . . . O10 O 0.68543(12) -0.65081(8) 0.41586(10) 0.0260(5) Uani 1 1 d . . . O11 O 0.75844(12) -0.74481(8) 0.35907(11) 0.0278(5) Uani 1 1 d . . . O12 O 0.81796(11) -0.63683(8) 0.33822(10) 0.0247(5) Uani 1 1 d . . . O13 O 0.62857(13) -0.78123(8) 0.41151(12) 0.0330(5) Uani 1 1 d . . . O14 O 0.71413(13) -0.84557(8) 0.36117(12) 0.0343(5) Uani 1 1 d . . . O15 O 0.57023(12) -0.82253(8) 0.26954(12) 0.0331(5) Uani 1 1 d . . . O16 O 0.46828(12) -0.77285(8) 0.23503(12) 0.0327(5) Uani 1 1 d . . . O17 O 0.51124(13) -0.74806(8) 0.37711(12) 0.0346(5) Uani 1 1 d . . . O18 O 0.52736(12) -0.64920(8) 0.34919(11) 0.0280(5) Uani 1 1 d . . . O19 O 0.53093(12) -0.55185(8) 0.31234(11) 0.0289(5) Uani 1 1 d . . . O20 O 0.58945(12) -0.57941(8) 0.45955(11) 0.0293(5) Uani 1 1 d . . . O21 O 0.69533(12) -0.54622(8) 0.39597(11) 0.0303(5) Uani 1 1 d . . . O22 O 0.56131(12) -0.52874(8) 0.21277(11) 0.0302(5) Uani 1 1 d . . . O23 O 0.71619(13) -0.51395(8) 0.29617(11) 0.0312(5) Uani 1 1 d . . . O24 O 0.76646(11) -0.58027(7) 0.21074(11) 0.0252(5) Uani 1 1 d . . . O25 O 0.92478(11) -0.60559(8) 0.26016(11) 0.0280(5) Uani 1 1 d . . . O26 O 0.83111(13) -0.64671(8) 0.13598(11) 0.0330(5) Uani 1 1 d . . . O27 O 0.89241(12) -0.70543(8) 0.25913(12) 0.0321(5) Uani 1 1 d . . . O28 O 0.79016(16) -0.85709(10) 0.47299(14) 0.0518(7) Uani 1 1 d . . . O29 O 0.65685(18) -0.56850(11) 0.57315(14) 0.0612(8) Uani 1 1 d . . . O30 O 1.01871(13) -0.63560(9) 0.35066(13) 0.0382(6) Uani 1 1 d . . . O31 O 0.61526(19) -0.43991(10) 0.00891(14) 0.0578(8) Uani 1 1 d . . . H31 H 0.6469 -0.4176 0.0074 0.087 Uiso 1 1 calc R . . O32 O 0.64960(14) -0.81600(9) -0.08520(12) 0.0376(6) Uani 1 1 d . . . H32 H 0.6081 -0.8287 -0.1087 0.056 Uiso 1 1 calc R . . O33 O 0.27014(15) -0.68238(11) 0.35553(15) 0.0538(7) Uani 1 1 d . . . H33 H 0.2286 -0.6859 0.3663 0.081 Uiso 1 1 calc R . . N1 N 0.66785(15) -0.79625(10) 0.08151(14) 0.0299(6) Uani 1 1 d . . . N2 N 0.39185(14) -0.68373(10) 0.26067(15) 0.0300(6) Uani 1 1 d . . . N3 N 0.65916(14) -0.52040(9) 0.12252(13) 0.0264(6) Uani 1 1 d . . . N4 N 0.83029(15) -0.68344(10) 0.46368(14) 0.0288(6) Uani 1 1 d . . . N5 N 0.2888(3) -0.2905(3) 0.3354(4) 0.147(3) Uani 1 1 d . . . C1 C 0.6445(2) -0.83722(13) 0.12279(19) 0.0393(9) Uani 1 1 d . . . H1B H 0.6464 -0.8689 0.0981 0.047 Uiso 1 1 calc R . . H1A H 0.5912 -0.8319 0.1252 0.047 Uiso 1 1 calc R . . C2 C 0.6979(2) -0.83880(12) 0.19735(18) 0.0346(8) Uani 1 1 d . . . H2B H 0.6801 -0.8636 0.2267 0.042 Uiso 1 1 calc R . . H2A H 0.7502 -0.8479 0.1955 0.042 Uiso 1 1 calc R . . C3 C 0.60004(18) -0.77106(13) 0.03438(17) 0.0324(8) Uani 1 1 d . . . H3B H 0.5639 -0.7958 0.0063 0.039 Uiso 1 1 calc R . . H3A H 0.6165 -0.7495 0.0001 0.039 Uiso 1 1 calc R . . C4 C 0.55992(18) -0.74058(13) 0.07898(18) 0.0337(8) Uani 1 1 d . . . H4B H 0.5224 -0.7181 0.0476 0.040 Uiso 1 1 calc R . . H4A H 0.5323 -0.7622 0.1046 0.040 Uiso 1 1 calc R . . C5 C 0.72066(19) -0.81451(13) 0.04063(18) 0.0337(8) Uani 1 1 d . . . H5B H 0.7617 -0.8340 0.0736 0.040 Uiso 1 1 calc R . . H5A H 0.7452 -0.7859 0.0244 0.040 Uiso 1 1 calc R . . C6 C 0.6837(2) -0.84587(13) -0.02426(18) 0.0384(8) Uani 1 1 d . . . H6B H 0.7230 -0.8674 -0.0354 0.046 Uiso 1 1 calc R . . H6A H 0.6440 -0.8670 -0.0133 0.046 Uiso 1 1 calc R . . C7 C 0.34221(18) -0.72028(13) 0.2849(2) 0.0351(8) Uani 1 1 d . . . H7B H 0.3700 -0.7313 0.3339 0.042 Uiso 1 1 calc R . . H7A H 0.3360 -0.7493 0.2530 0.042 Uiso 1 1 calc R . . C8 C 0.2634(2) -0.70342(14) 0.28652(19) 0.0383(8) Uani 1 1 d . . . H8B H 0.2436 -0.6787 0.2484 0.046 Uiso 1 1 calc R . . H8A H 0.2276 -0.7316 0.2783 0.046 Uiso 1 1 calc R . . C9 C 0.39446(18) -0.63541(12) 0.29736(18) 0.0321(7) Uani 1 1 d . . . H9B H 0.3446 -0.6288 0.3073 0.039 Uiso 1 1 calc R . . H9A H 0.4043 -0.6089 0.2660 0.039 Uiso 1 1 calc R . . C10 C 0.45738(17) -0.63642(13) 0.36670(18) 0.0310(7) Uani 1 1 d . . . H10B H 0.4625 -0.6038 0.3903 0.037 Uiso 1 1 calc R . . H10A H 0.4457 -0.6610 0.3999 0.037 Uiso 1 1 calc R . . C11 C 0.37040(18) -0.67820(14) 0.18145(18) 0.0367(8) Uani 1 1 d . . . H11B H 0.3237 -0.6577 0.1656 0.044 Uiso 1 1 calc R . . H11A H 0.3590 -0.7109 0.1584 0.044 Uiso 1 1 calc R . . C12 C 0.43605(18) -0.65415(13) 0.15836(18) 0.0352(8) Uani 1 1 d . . . H12B H 0.4281 -0.6583 0.1060 0.042 Uiso 1 1 calc R . . H12A H 0.4381 -0.6186 0.1693 0.042 Uiso 1 1 calc R . . C13 C 0.73328(18) -0.53020(12) 0.10550(17) 0.0305(7) Uani 1 1 d . . . H13B H 0.7484 -0.5011 0.0819 0.037 Uiso 1 1 calc R . . H13A H 0.7273 -0.5584 0.0720 0.037 Uiso 1 1 calc R . . C14 C 0.79456(18) -0.54157(12) 0.17416(17) 0.0292(7) Uani 1 1 d . . . H14B H 0.8423 -0.5521 0.1630 0.035 Uiso 1 1 calc R . . H14A H 0.8059 -0.5119 0.2050 0.035 Uiso 1 1 calc R . . C15 C 0.59364(19) -0.54270(12) 0.06776(17) 0.0315(7) Uani 1 1 d . . . H15B H 0.5963 -0.5333 0.0190 0.038 Uiso 1 1 calc R . . H15A H 0.5448 -0.5301 0.0744 0.038 Uiso 1 1 calc R . . C16 C 0.5957(2) -0.59841(12) 0.07461(16) 0.0339(8) Uani 1 1 d . . . H16B H 0.5470 -0.6127 0.0451 0.041 Uiso 1 1 calc R . . H16A H 0.6384 -0.6120 0.0578 0.041 Uiso 1 1 calc R . . C17 C 0.6491(2) -0.46664(12) 0.13486(18) 0.0334(8) Uani 1 1 d . . . H17B H 0.7004 -0.4511 0.1462 0.040 Uiso 1 1 calc R . . H17A H 0.6303 -0.4634 0.1781 0.040 Uiso 1 1 calc R . . C18 C 0.5963(2) -0.43738(15) 0.0755(2) 0.0482(10) Uani 1 1 d . . . H18B H 0.5432 -0.4495 0.0682 0.058 Uiso 1 1 calc R . . H18A H 0.5976 -0.4026 0.0906 0.058 Uiso 1 1 calc R . . C19 C 0.84400(19) -0.73655(12) 0.47448(17) 0.0329(8) Uani 1 1 d . . . H19B H 0.8074 -0.7509 0.4986 0.040 Uiso 1 1 calc R . . H19A H 0.8968 -0.7426 0.5049 0.040 Uiso 1 1 calc R . . C20 C 0.83317(18) -0.75961(12) 0.40161(17) 0.0312(7) Uani 1 1 d . . . H20B H 0.8732 -0.7480 0.3794 0.037 Uiso 1 1 calc R . . H20A H 0.8363 -0.7959 0.4057 0.037 Uiso 1 1 calc R . . C21 C 0.79453(19) -0.66117(13) 0.51584(17) 0.0338(8) Uani 1 1 d . . . H21B H 0.8075 -0.6258 0.5215 0.041 Uiso 1 1 calc R . . H21A H 0.8139 -0.6773 0.5633 0.041 Uiso 1 1 calc R . . C22 C 0.70842(19) -0.66764(13) 0.48854(16) 0.0319(7) Uani 1 1 d . . . H22B H 0.6946 -0.7027 0.4909 0.038 Uiso 1 1 calc R . . H22A H 0.6824 -0.6483 0.5183 0.038 Uiso 1 1 calc R . . C23 C 0.89686(18) -0.65612(12) 0.45434(18) 0.0319(7) Uani 1 1 d . . . H23B H 0.9306 -0.6782 0.4360 0.038 Uiso 1 1 calc R . . H23A H 0.9269 -0.6424 0.5010 0.038 Uiso 1 1 calc R . . C24 C 0.86723(18) -0.61500(12) 0.40116(16) 0.0279(7) Uani 1 1 d . . . H24B H 0.8385 -0.5907 0.4218 0.033 Uiso 1 1 calc R . . H24A H 0.9105 -0.5980 0.3893 0.033 Uiso 1 1 calc R . . C25 C 0.88609(18) -0.74853(12) 0.23599(17) 0.0285(7) Uani 1 1 d . . . C26 C 0.9510(2) -0.78316(13) 0.26717(19) 0.0349(8) Uani 1 1 d . . . C27 C 1.0180(2) -0.76537(16) 0.3125(2) 0.0570(12) Uani 1 1 d . . . H27A H 1.0229 -0.7312 0.3230 0.068 Uiso 1 1 calc R . . C28 C 1.0782(3) -0.7968(2) 0.3431(3) 0.0867(19) Uani 1 1 d . . . H28A H 1.1248 -0.7842 0.3734 0.104 Uiso 1 1 calc R . . C29 C 1.0702(3) -0.8464(2) 0.3293(3) 0.0873(19) Uani 1 1 d . . . H29A H 1.1110 -0.8681 0.3510 0.105 Uiso 1 1 calc R . . C30 C 1.0037(3) -0.86460(18) 0.2845(3) 0.0752(15) Uani 1 1 d . . . H30A H 0.9986 -0.8989 0.2754 0.090 Uiso 1 1 calc R . . C31 C 0.9437(2) -0.83314(14) 0.2523(2) 0.0515(10) Uani 1 1 d . . . H31A H 0.8981 -0.8457 0.2204 0.062 Uiso 1 1 calc R . . C32 C 0.79658(17) -0.67041(11) 0.08025(17) 0.0264(7) Uani 1 1 d . . . C33 C 0.81581(18) -0.65723(12) 0.01190(16) 0.0290(7) Uani 1 1 d . . . C34 C 0.8710(2) -0.62222(14) 0.0127(2) 0.0465(10) Uani 1 1 d . . . H34A H 0.8940 -0.6050 0.0560 0.056 Uiso 1 1 calc R . . C35 C 0.8932(3) -0.61181(16) -0.0487(2) 0.0545(11) Uani 1 1 d . . . H35A H 0.9314 -0.5877 -0.0474 0.065 Uiso 1 1 calc R . . C36 C 0.8600(2) -0.63639(15) -0.1114(2) 0.0473(10) Uani 1 1 d . . . H36A H 0.8756 -0.6296 -0.1535 0.057 Uiso 1 1 calc R . . C37 C 0.8042(2) -0.67080(15) -0.11313(19) 0.0453(9) Uani 1 1 d . . . H37A H 0.7804 -0.6872 -0.1569 0.054 Uiso 1 1 calc R . . C38 C 0.7821(2) -0.68189(14) -0.05171(18) 0.0381(8) Uani 1 1 d . . . H38A H 0.7441 -0.7062 -0.0532 0.046 Uiso 1 1 calc R . . C39 C 0.50011(19) -0.81441(12) 0.24206(17) 0.0290(7) Uani 1 1 d . . . C40 C 0.45024(19) -0.85879(12) 0.21652(17) 0.0308(7) Uani 1 1 d . . . C41 C 0.3711(2) -0.85504(13) 0.20067(17) 0.0350(8) Uani 1 1 d . . . H41A H 0.3480 -0.8241 0.2035 0.042 Uiso 1 1 calc R . . C42 C 0.3254(2) -0.89668(14) 0.18063(19) 0.0438(9) Uani 1 1 d . . . H42A H 0.2712 -0.8941 0.1694 0.053 Uiso 1 1 calc R . . C43 C 0.3589(2) -0.94125(15) 0.1772(2) 0.0496(10) Uani 1 1 d . . . H43A H 0.3277 -0.9696 0.1636 0.060 Uiso 1 1 calc R . . C44 C 0.4372(3) -0.94561(15) 0.1932(2) 0.0543(11) Uani 1 1 d . . . H44A H 0.4600 -0.9768 0.1914 0.065 Uiso 1 1 calc R . . C45 C 0.4828(2) -0.90419(13) 0.2120(2) 0.0445(9) Uani 1 1 d . . . H45A H 0.5369 -0.9070 0.2220 0.053 Uiso 1 1 calc R . . C46 C 0.62142(19) -0.55150(14) 0.51385(18) 0.0360(8) Uani 1 1 d . . . C47 C 0.6148(2) -0.49757(14) 0.50401(19) 0.0370(8) Uani 1 1 d . . . C48 C 0.6573(2) -0.46679(15) 0.5583(2) 0.0464(10) Uani 1 1 d . . . H48A H 0.6877 -0.4804 0.6021 0.056 Uiso 1 1 calc R . . C49 C 0.6549(3) -0.41703(17) 0.5481(3) 0.0593(12) Uani 1 1 d . . . H49A H 0.6844 -0.3962 0.5847 0.071 Uiso 1 1 calc R . . C50 C 0.6098(3) -0.39654(17) 0.4849(3) 0.0659(13) Uani 1 1 d . . . H50A H 0.6085 -0.3619 0.4783 0.079 Uiso 1 1 calc R . . C51 C 0.5670(3) -0.42699(16) 0.4319(3) 0.0675(14) Uani 1 1 d . . . H51A H 0.5358 -0.4135 0.3883 0.081 Uiso 1 1 calc R . . C52 C 0.5696(2) -0.47727(15) 0.4425(2) 0.0509(10) Uani 1 1 d . . . H52A H 0.5393 -0.4981 0.4063 0.061 Uiso 1 1 calc R . . C53 C 0.73223(18) -0.51987(11) 0.36387(17) 0.0279(7) Uani 1 1 d . . . C54 C 0.80206(18) -0.49423(11) 0.40948(17) 0.0281(7) Uani 1 1 d . . . C55 C 0.8573(2) -0.47581(12) 0.37921(19) 0.0359(8) Uani 1 1 d . . . H55A H 0.8491 -0.4764 0.3285 0.043 Uiso 1 1 calc R . . C56 C 0.9248(2) -0.45648(14) 0.4232(2) 0.0452(9) Uani 1 1 d . . . H56A H 0.9633 -0.4446 0.4025 0.054 Uiso 1 1 calc R . . C57 C 0.9363(2) -0.45436(13) 0.4963(2) 0.0437(9) Uani 1 1 d . . . H57A H 0.9821 -0.4404 0.5260 0.052 Uiso 1 1 calc R . . C58 C 0.8817(2) -0.47233(14) 0.5264(2) 0.0426(9) Uani 1 1 d . . . H58A H 0.8898 -0.4707 0.5770 0.051 Uiso 1 1 calc R . . C59 C 0.8149(2) -0.49284(13) 0.48391(19) 0.0365(8) Uani 1 1 d . . . H59A H 0.7778 -0.5060 0.5053 0.044 Uiso 1 1 calc R . . C60 C 0.51696(17) -0.53015(11) 0.25257(16) 0.0256(7) Uani 1 1 d . . . C61 C 0.44092(18) -0.50493(11) 0.22613(17) 0.0275(7) Uani 1 1 d . . . C62 C 0.40090(19) -0.48999(13) 0.27452(19) 0.0351(8) Uani 1 1 d . . . H62A H 0.4210 -0.4966 0.3244 0.042 Uiso 1 1 calc R . . C63 C 0.3320(2) -0.46559(14) 0.2500(2) 0.0442(9) Uani 1 1 d . . . H63A H 0.3055 -0.4546 0.2832 0.053 Uiso 1 1 calc R . . C64 C 0.3012(2) -0.45708(14) 0.1775(2) 0.0460(10) Uani 1 1 d . . . H64A H 0.2539 -0.4401 0.1610 0.055 Uiso 1 1 calc R . . C65 C 0.3390(2) -0.47316(15) 0.1289(2) 0.0483(10) Uani 1 1 d . . . H65A H 0.3170 -0.4679 0.0789 0.058 Uiso 1 1 calc R . . C66 C 0.4091(2) -0.49698(13) 0.15268(19) 0.0379(8) Uani 1 1 d . . . H66A H 0.4353 -0.5078 0.1191 0.046 Uiso 1 1 calc R . . C67 C 0.7314(2) -0.86640(12) 0.4245(2) 0.0362(8) Uani 1 1 d . . . C68 C 0.6788(2) -0.90608(13) 0.4355(2) 0.0387(8) Uani 1 1 d . . . C69 C 0.6982(2) -0.93393(13) 0.4990(2) 0.0410(9) Uani 1 1 d . . . H69A H 0.7431 -0.9262 0.5362 0.049 Uiso 1 1 calc R . . C70 C 0.6520(2) -0.97248(15) 0.5073(2) 0.0475(10) Uani 1 1 d . . . H70A H 0.6659 -0.9918 0.5498 0.057 Uiso 1 1 calc R . . C71 C 0.5855(2) -0.98321(14) 0.4542(2) 0.0486(10) Uani 1 1 d . . . H71A H 0.5538 -1.0098 0.4603 0.058 Uiso 1 1 calc R . . C72 C 0.5653(3) -0.95516(16) 0.3924(2) 0.0582(12) Uani 1 1 d . . . H72A H 0.5195 -0.9622 0.3560 0.070 Uiso 1 1 calc R . . C73 C 0.6125(2) -0.91655(14) 0.3835(2) 0.0478(10) Uani 1 1 d . . . H73A H 0.5984 -0.8973 0.3409 0.057 Uiso 1 1 calc R . . C74 C 0.56578(19) -0.76909(12) 0.42263(18) 0.0303(7) Uani 1 1 d . . . C75 C 0.5527(2) -0.78023(13) 0.49433(18) 0.0339(8) Uani 1 1 d . . . C76 C 0.4872(2) -0.76261(14) 0.5109(2) 0.0442(9) Uani 1 1 d . . . H76A H 0.4504 -0.7442 0.4761 0.053 Uiso 1 1 calc R . . C77 C 0.4757(3) -0.77171(16) 0.5772(2) 0.0543(11) Uani 1 1 d . . . H77A H 0.4322 -0.7583 0.5888 0.065 Uiso 1 1 calc R . . C78 C 0.5269(3) -0.80004(16) 0.6266(2) 0.0560(12) Uani 1 1 d . . . H78A H 0.5180 -0.8070 0.6719 0.067 Uiso 1 1 calc R . . C79 C 0.5914(3) -0.81855(17) 0.6105(2) 0.0583(12) Uani 1 1 d . . . H79A H 0.6265 -0.8384 0.6446 0.070 Uiso 1 1 calc R . . C80 C 0.6053(2) -0.80828(15) 0.5447(2) 0.0458(9) Uani 1 1 d . . . H80A H 0.6503 -0.8203 0.5343 0.055 Uiso 1 1 calc R . . C81 C 0.99581(18) -0.61276(12) 0.29361(17) 0.0280(7) Uani 1 1 d . . . C82 C 1.05299(18) -0.59031(12) 0.25931(17) 0.0290(7) Uani 1 1 d . . . C83 C 1.0294(2) -0.57221(15) 0.1898(2) 0.0444(9) Uani 1 1 d . . . H83A H 0.9765 -0.5727 0.1643 0.053 Uiso 1 1 calc R . . C84 C 1.0828(2) -0.55338(19) 0.1573(2) 0.0611(13) Uani 1 1 d . . . H84A H 1.0665 -0.5412 0.1095 0.073 Uiso 1 1 calc R . . C85 C 1.1596(2) -0.55234(15) 0.1942(2) 0.0470(10) Uani 1 1 d . . . H85A H 1.1961 -0.5398 0.1717 0.056 Uiso 1 1 calc R . . C86 C 1.1831(2) -0.56933(13) 0.2631(2) 0.0393(8) Uani 1 1 d . . . H86A H 1.2358 -0.5681 0.2888 0.047 Uiso 1 1 calc R . . C87 C 1.13032(18) -0.58832(12) 0.29547(19) 0.0342(8) Uani 1 1 d . . . H87A H 1.1473 -0.6002 0.3434 0.041 Uiso 1 1 calc R . . C88 C 0.3441(4) -0.3118(2) 0.3492(3) 0.0821(18) Uani 1 1 d . . . C89 C 0.4143(4) -0.3375(2) 0.3708(4) 0.109(2) Uani 1 1 d . . . H89C H 0.4123 -0.3660 0.3394 0.163 Uiso 1 1 calc R . . H89B H 0.4230 -0.3486 0.4206 0.163 Uiso 1 1 calc R . . H89A H 0.4562 -0.3157 0.3674 0.163 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0223(2) 0.0255(2) 0.0248(2) -0.00330(18) 0.00668(18) -0.00208(18) Fe2 0.0201(2) 0.0241(2) 0.0221(2) -0.00003(17) 0.00550(17) -0.00146(17) Fe3 0.0216(2) 0.0251(2) 0.0239(2) 0.00101(18) 0.00693(18) 0.00053(18) Fe4 0.0259(2) 0.0241(2) 0.0271(2) 0.00176(18) 0.00811(19) -0.00069(18) Fe5 0.0216(2) 0.0250(2) 0.0288(2) 0.00060(19) 0.00878(19) -0.00206(18) Fe6 0.0210(2) 0.0248(2) 0.0218(2) -0.00011(17) 0.00610(17) 0.00017(17) Fe7 0.0209(2) 0.0236(2) 0.0216(2) 0.00165(17) 0.00591(17) -0.00049(17) Fe8 0.0192(2) 0.0251(2) 0.0224(2) -0.00091(17) 0.00613(17) -0.00142(17) O1 0.0359(13) 0.0242(11) 0.0303(12) -0.0013(9) 0.0129(10) -0.0012(10) O2 0.0309(12) 0.0339(13) 0.0268(12) -0.0010(10) 0.0083(10) -0.0083(10) O3 0.0225(11) 0.0313(12) 0.0261(11) -0.0059(9) 0.0048(9) -0.0039(9) O4 0.0192(10) 0.0244(11) 0.0239(11) -0.0011(8) 0.0066(8) -0.0016(8) O5 0.0264(12) 0.0338(13) 0.0352(13) -0.0063(10) 0.0058(10) 0.0009(10) O6 0.0282(12) 0.0275(12) 0.0199(11) 0.0025(9) 0.0037(9) -0.0020(9) O7 0.0194(11) 0.0300(12) 0.0297(12) 0.0035(9) 0.0053(9) -0.0004(9) O8 0.0233(11) 0.0226(11) 0.0244(11) 0.0009(9) 0.0083(9) -0.0004(8) O9 0.0197(10) 0.0235(11) 0.0232(11) 0.0013(8) 0.0063(8) 0.0000(8) O10 0.0267(11) 0.0318(12) 0.0199(11) 0.0031(9) 0.0070(9) 0.0043(9) O11 0.0263(12) 0.0273(12) 0.0284(12) 0.0010(9) 0.0052(9) -0.0001(9) O12 0.0220(11) 0.0298(12) 0.0208(10) -0.0026(9) 0.0035(9) -0.0027(9) O13 0.0332(13) 0.0358(13) 0.0327(13) 0.0043(10) 0.0136(10) 0.0020(10) O14 0.0389(14) 0.0280(12) 0.0370(13) 0.0050(10) 0.0122(11) 0.0044(10) O15 0.0274(12) 0.0271(12) 0.0436(14) -0.0026(10) 0.0075(10) -0.0035(10) O16 0.0292(12) 0.0304(13) 0.0373(13) -0.0022(10) 0.0068(10) -0.0031(10) O17 0.0312(13) 0.0366(13) 0.0380(13) 0.0088(11) 0.0131(11) 0.0000(10) O18 0.0211(11) 0.0308(12) 0.0334(12) -0.0036(10) 0.0099(9) -0.0011(9) O19 0.0283(12) 0.0331(12) 0.0256(12) 0.0032(9) 0.0079(9) 0.0058(10) O20 0.0285(12) 0.0351(13) 0.0257(12) -0.0035(10) 0.0094(10) -0.0016(10) O21 0.0284(12) 0.0341(13) 0.0291(12) -0.0045(10) 0.0089(10) -0.0067(10) O22 0.0257(12) 0.0346(13) 0.0314(12) 0.0070(10) 0.0098(10) 0.0058(10) O23 0.0363(13) 0.0292(12) 0.0279(12) -0.0024(9) 0.0083(10) -0.0040(10) O24 0.0231(11) 0.0276(11) 0.0266(11) 0.0073(9) 0.0098(9) -0.0018(9) O25 0.0202(11) 0.0305(12) 0.0315(12) -0.0007(9) 0.0040(9) -0.0033(9) O26 0.0344(13) 0.0426(14) 0.0247(12) -0.0063(10) 0.0126(10) -0.0108(11) O27 0.0253(12) 0.0288(12) 0.0407(13) -0.0026(10) 0.0067(10) 0.0026(9) O28 0.0563(18) 0.0480(17) 0.0437(16) 0.0068(13) 0.0011(14) -0.0047(14) O29 0.076(2) 0.0628(19) 0.0327(15) -0.0050(14) -0.0047(14) 0.0164(16) O30 0.0277(13) 0.0497(15) 0.0357(13) 0.0087(12) 0.0059(10) -0.0011(11) O31 0.081(2) 0.0479(18) 0.0401(16) 0.0075(13) 0.0086(15) -0.0110(15) O32 0.0361(14) 0.0447(15) 0.0300(13) -0.0056(11) 0.0056(10) -0.0036(11) O33 0.0456(17) 0.0670(19) 0.0551(17) -0.0206(15) 0.0244(14) -0.0106(15) N1 0.0297(15) 0.0330(15) 0.0270(14) -0.0046(12) 0.0080(12) -0.0046(12) N2 0.0222(14) 0.0319(15) 0.0359(15) -0.0015(12) 0.0081(12) -0.0032(11) N3 0.0249(14) 0.0279(14) 0.0257(14) 0.0056(11) 0.0056(11) 0.0005(11) N4 0.0258(14) 0.0329(15) 0.0268(14) 0.0022(11) 0.0059(11) 0.0032(11) N5 0.076(4) 0.159(6) 0.170(6) 0.117(5) -0.024(4) -0.038(4) C1 0.051(2) 0.0307(19) 0.039(2) -0.0073(15) 0.0179(17) -0.0136(16) C2 0.049(2) 0.0236(17) 0.0356(19) -0.0024(14) 0.0184(16) -0.0014(15) C3 0.0281(17) 0.0382(19) 0.0281(17) -0.0089(14) 0.0034(14) -0.0055(14) C4 0.0226(17) 0.042(2) 0.0325(18) -0.0097(15) 0.0005(14) -0.0053(14) C5 0.0348(19) 0.0354(19) 0.0315(18) -0.0052(15) 0.0101(15) 0.0022(15) C6 0.048(2) 0.035(2) 0.0325(19) -0.0060(15) 0.0110(16) 0.0018(16) C7 0.0266(18) 0.0346(19) 0.047(2) -0.0016(16) 0.0147(16) -0.0064(14) C8 0.0320(19) 0.043(2) 0.042(2) -0.0102(17) 0.0140(16) -0.0062(16) C9 0.0232(17) 0.0290(17) 0.047(2) -0.0028(15) 0.0140(15) 0.0007(13) C10 0.0226(16) 0.0356(19) 0.0383(19) -0.0060(15) 0.0142(14) -0.0033(14) C11 0.0216(17) 0.048(2) 0.038(2) -0.0018(16) 0.0048(14) -0.0015(15) C12 0.0227(17) 0.048(2) 0.0320(18) 0.0058(16) 0.0027(14) 0.0034(15) C13 0.0342(18) 0.0304(18) 0.0299(17) 0.0043(14) 0.0138(14) -0.0004(14) C14 0.0259(17) 0.0299(17) 0.0347(18) 0.0071(14) 0.0132(14) -0.0030(13) C15 0.0326(18) 0.0360(19) 0.0227(16) 0.0043(14) 0.0023(14) -0.0026(14) C16 0.042(2) 0.0359(19) 0.0219(16) 0.0011(14) 0.0051(15) -0.0067(15) C17 0.039(2) 0.0284(18) 0.0343(18) 0.0071(14) 0.0122(15) 0.0018(15) C18 0.050(2) 0.042(2) 0.051(2) 0.0050(18) 0.010(2) 0.0033(18) C19 0.0294(18) 0.0367(19) 0.0299(18) 0.0068(15) 0.0035(14) 0.0067(15) C20 0.0235(17) 0.0308(18) 0.0373(19) 0.0045(14) 0.0047(14) 0.0036(13) C21 0.039(2) 0.0393(19) 0.0225(16) 0.0007(14) 0.0079(14) 0.0048(15) C22 0.0352(19) 0.0385(19) 0.0232(16) 0.0060(14) 0.0102(14) 0.0059(15) C23 0.0219(16) 0.0389(19) 0.0313(18) -0.0024(15) 0.0011(14) -0.0004(14) C24 0.0249(16) 0.0326(17) 0.0247(16) -0.0034(13) 0.0044(13) -0.0031(13) C25 0.0280(17) 0.0326(18) 0.0276(17) -0.0006(14) 0.0124(14) 0.0033(14) C26 0.0323(19) 0.0349(19) 0.0388(19) -0.0037(15) 0.0121(15) 0.0089(15) C27 0.046(2) 0.053(3) 0.060(3) -0.017(2) -0.007(2) 0.018(2) C28 0.056(3) 0.085(4) 0.091(4) -0.033(3) -0.027(3) 0.041(3) C29 0.077(4) 0.080(4) 0.084(4) -0.011(3) -0.014(3) 0.053(3) C30 0.080(4) 0.048(3) 0.089(4) -0.005(3) 0.009(3) 0.034(3) C31 0.050(2) 0.037(2) 0.065(3) -0.0059(19) 0.010(2) 0.0100(18) C32 0.0238(16) 0.0280(17) 0.0278(16) -0.0008(13) 0.0076(13) 0.0022(13) C33 0.0302(17) 0.0334(18) 0.0242(16) -0.0017(13) 0.0090(14) 0.0021(14) C34 0.067(3) 0.046(2) 0.032(2) -0.0086(17) 0.0231(19) -0.020(2) C35 0.074(3) 0.051(3) 0.048(2) -0.002(2) 0.033(2) -0.021(2) C36 0.064(3) 0.052(2) 0.032(2) 0.0090(18) 0.0249(19) 0.010(2) C37 0.055(2) 0.054(2) 0.0267(19) -0.0037(17) 0.0098(17) 0.001(2) C38 0.037(2) 0.046(2) 0.0284(18) -0.0027(16) 0.0050(15) -0.0035(16) C39 0.0356(19) 0.0287(17) 0.0242(16) -0.0011(13) 0.0107(14) -0.0067(14) C40 0.0362(19) 0.0301(18) 0.0255(16) 0.0001(13) 0.0073(14) -0.0073(14) C41 0.038(2) 0.0356(19) 0.0299(18) 0.0015(15) 0.0059(15) -0.0084(15) C42 0.041(2) 0.051(2) 0.036(2) -0.0010(17) 0.0057(17) -0.0176(18) C43 0.056(3) 0.041(2) 0.049(2) -0.0049(18) 0.009(2) -0.0203(19) C44 0.067(3) 0.034(2) 0.058(3) -0.0063(19) 0.010(2) -0.007(2) C45 0.047(2) 0.036(2) 0.049(2) -0.0088(17) 0.0092(18) -0.0046(17) C46 0.0295(18) 0.051(2) 0.0279(18) -0.0053(16) 0.0087(15) 0.0020(16) C47 0.0333(19) 0.044(2) 0.038(2) -0.0076(16) 0.0155(16) -0.0020(16) C48 0.039(2) 0.055(3) 0.047(2) -0.0165(19) 0.0166(18) -0.0072(18) C49 0.058(3) 0.066(3) 0.064(3) -0.030(2) 0.033(2) -0.017(2) C50 0.088(4) 0.040(3) 0.081(4) -0.013(2) 0.044(3) -0.006(2) C51 0.096(4) 0.044(3) 0.059(3) -0.003(2) 0.016(3) 0.016(3) C52 0.059(3) 0.042(2) 0.049(2) -0.0105(19) 0.010(2) 0.007(2) C53 0.0267(17) 0.0244(16) 0.0323(18) -0.0032(13) 0.0076(14) 0.0023(13) C54 0.0290(17) 0.0244(16) 0.0310(17) -0.0018(13) 0.0082(14) -0.0003(13) C55 0.039(2) 0.0302(18) 0.038(2) 0.0020(15) 0.0096(16) -0.0069(15) C56 0.030(2) 0.042(2) 0.061(3) 0.0045(19) 0.0082(18) -0.0074(16) C57 0.033(2) 0.035(2) 0.053(2) -0.0034(17) -0.0052(18) -0.0038(16) C58 0.039(2) 0.045(2) 0.039(2) -0.0071(17) 0.0020(17) 0.0030(17) C59 0.0324(19) 0.040(2) 0.037(2) -0.0065(16) 0.0094(15) -0.0036(15) C60 0.0254(16) 0.0223(16) 0.0288(17) -0.0008(13) 0.0070(13) -0.0003(12) C61 0.0258(17) 0.0245(16) 0.0306(17) 0.0016(13) 0.0050(13) 0.0006(13) C62 0.0309(18) 0.040(2) 0.0337(19) -0.0030(15) 0.0073(15) 0.0029(15) C63 0.034(2) 0.044(2) 0.057(2) -0.0076(19) 0.0177(18) 0.0083(17) C64 0.0272(19) 0.041(2) 0.067(3) 0.0094(19) 0.0086(19) 0.0105(16) C65 0.034(2) 0.059(3) 0.046(2) 0.0161(19) 0.0010(18) 0.0085(18) C66 0.0316(19) 0.047(2) 0.0343(19) 0.0069(16) 0.0080(15) 0.0065(16) C67 0.044(2) 0.0264(18) 0.040(2) 0.0019(15) 0.0155(17) 0.0080(15) C68 0.047(2) 0.0315(19) 0.040(2) -0.0022(16) 0.0173(17) 0.0064(16) C69 0.054(2) 0.036(2) 0.036(2) -0.0008(16) 0.0176(18) 0.0051(17) C70 0.063(3) 0.045(2) 0.042(2) 0.0079(18) 0.028(2) 0.007(2) C71 0.054(3) 0.039(2) 0.059(3) 0.0061(19) 0.026(2) -0.0023(19) C72 0.052(3) 0.053(3) 0.064(3) 0.011(2) 0.006(2) -0.010(2) C73 0.052(2) 0.041(2) 0.047(2) 0.0132(18) 0.010(2) -0.0011(19) C74 0.0316(18) 0.0285(17) 0.0316(18) 0.0007(14) 0.0099(15) -0.0052(14) C75 0.039(2) 0.0338(19) 0.0316(18) -0.0020(15) 0.0136(15) -0.0102(15) C76 0.044(2) 0.047(2) 0.046(2) 0.0058(18) 0.0194(18) -0.0053(18) C77 0.062(3) 0.060(3) 0.053(3) -0.001(2) 0.036(2) -0.009(2) C78 0.074(3) 0.064(3) 0.036(2) 0.003(2) 0.025(2) -0.019(2) C79 0.066(3) 0.068(3) 0.035(2) 0.013(2) 0.005(2) -0.004(2) C80 0.048(2) 0.052(2) 0.039(2) 0.0069(18) 0.0138(18) -0.0026(19) C81 0.0270(17) 0.0279(17) 0.0285(17) -0.0035(13) 0.0064(14) -0.0015(13) C82 0.0237(16) 0.0295(17) 0.0337(18) -0.0030(14) 0.0080(14) -0.0022(13) C83 0.0252(18) 0.069(3) 0.037(2) 0.0105(19) 0.0044(15) -0.0008(18) C84 0.037(2) 0.102(4) 0.046(2) 0.027(2) 0.0132(19) 0.001(2) C85 0.034(2) 0.056(3) 0.056(3) 0.011(2) 0.0210(19) -0.0026(18) C86 0.0240(18) 0.045(2) 0.047(2) 0.0045(17) 0.0064(16) -0.0046(15) C87 0.0258(17) 0.0382(19) 0.0362(19) 0.0022(15) 0.0046(15) 0.0001(14) C88 0.071(4) 0.094(4) 0.068(3) 0.034(3) -0.003(3) -0.033(3) C89 0.091(5) 0.093(5) 0.159(7) -0.012(5) 0.063(5) -0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O4 1.938(2) . ? Fe1 O3 1.975(2) . ? Fe1 O5 1.996(2) . ? Fe1 O1 2.011(2) . ? Fe1 O2 2.074(2) . ? Fe1 N1 2.265(3) . ? Fe2 O3 1.939(2) . ? Fe2 O6 1.941(2) . ? Fe2 O7 1.952(2) . ? Fe2 O9 2.040(2) . ? Fe2 O8 2.065(2) . ? Fe2 O4 2.095(2) . ? Fe2 Fe3 2.9093(6) . ? Fe2 Fe5 2.9701(6) . ? Fe2 Fe7 2.9758(6) . ? Fe3 O10 1.929(2) . ? Fe3 O11 1.934(2) . ? Fe3 O12 1.939(2) . ? Fe3 O9 2.234(2) . ? Fe3 O4 2.238(2) . ? Fe3 O8 2.254(2) . ? Fe4 O11 1.954(2) . ? Fe4 O14 1.986(2) . ? Fe4 O8 1.991(2) . ? Fe4 O1 1.997(2) . ? Fe4 O15 2.032(2) . ? Fe4 O13 2.092(2) . ? Fe5 O8 1.946(2) . ? Fe5 O18 1.981(2) . ? Fe5 O7 1.986(2) . ? Fe5 O17 1.989(2) . ? Fe5 O16 2.074(2) . ? Fe5 N2 2.252(3) . ? Fe6 O20 1.957(2) . ? Fe6 O10 1.968(2) . ? Fe6 O18 1.984(2) . ? Fe6 O9 2.012(2) . ? Fe6 O19 2.043(2) . ? Fe6 O21 2.072(2) . ? Fe7 O9 1.952(2) . ? Fe7 O6 1.980(2) . ? Fe7 O24 1.993(2) . ? Fe7 O23 2.003(2) . ? Fe7 O22 2.050(2) . ? Fe7 N3 2.269(2) . ? Fe8 O12 1.968(2) . ? Fe8 O4 1.985(2) . ? Fe8 O24 1.992(2) . ? Fe8 O25 1.996(2) . ? Fe8 O26 2.023(2) . ? Fe8 O27 2.078(2) . ? O1 C2 1.423(4) . ? O2 C32 1.255(4) . ? O3 C4 1.409(3) . ? O5 C25 1.265(4) . ? O6 C16 1.418(4) . ? O7 C12 1.419(4) . ? O10 C22 1.428(4) . ? O11 C20 1.436(4) . ? O12 C24 1.427(3) . ? O13 C74 1.259(4) . ? O14 C67 1.307(4) . ? O15 C39 1.256(4) . ? O16 C39 1.260(4) . ? O17 C74 1.266(4) . ? O18 C10 1.442(4) . ? O19 C60 1.260(4) . ? O20 C46 1.297(4) . ? O21 C53 1.255(4) . ? O22 C60 1.256(4) . ? O23 C53 1.271(4) . ? O24 C14 1.437(3) . ? O25 C81 1.287(4) . ? O26 C32 1.265(4) . ? O27 C25 1.249(4) . ? O28 C67 1.238(4) . ? O29 C46 1.240(4) . ? O30 C81 1.235(4) . ? O31 C18 1.421(5) . ? O31 H31 0.8400 . ? O32 C6 1.426(4) . ? O32 H32 0.8400 . ? O33 C8 1.426(4) . ? O33 H33 0.8400 . ? N1 C3 1.482(4) . ? N1 C5 1.484(4) . ? N1 C1 1.498(4) . ? N2 C11 1.482(4) . ? N2 C9 1.489(4) . ? N2 C7 1.500(4) . ? N3 C15 1.487(4) . ? N3 C13 1.492(4) . ? N3 C17 1.501(4) . ? N4 C23 1.470(4) . ? N4 C21 1.470(4) . ? N4 C19 1.472(4) . ? N5 C88 1.123(8) . ? C1 C2 1.501(5) . ? C1 H1B 0.9900 . ? C1 H1A 0.9900 . ? C2 H2B 0.9900 . ? C2 H2A 0.9900 . ? C3 C4 1.518(4) . ? C3 H3B 0.9900 . ? C3 H3A 0.9900 . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C5 C6 1.514(4) . ? C5 H5B 0.9900 . ? C5 H5A 0.9900 . ? C6 H6B 0.9900 . ? C6 H6A 0.9900 . ? C7 C8 1.507(5) . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? C8 H8B 0.9900 . ? C8 H8A 0.9900 . ? C9 C10 1.504(4) . ? C9 H9B 0.9900 . ? C9 H9A 0.9900 . ? C10 H10B 0.9900 . ? C10 H10A 0.9900 . ? C11 C12 1.528(5) . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? C12 H12B 0.9900 . ? C12 H12A 0.9900 . ? C13 C14 1.512(4) . ? C13 H13B 0.9900 . ? C13 H13A 0.9900 . ? C14 H14B 0.9900 . ? C14 H14A 0.9900 . ? C15 C16 1.522(5) . ? C15 H15B 0.9900 . ? C15 H15A 0.9900 . ? C16 H16B 0.9900 . ? C16 H16A 0.9900 . ? C17 C18 1.505(5) . ? C17 H17B 0.9900 . ? C17 H17A 0.9900 . ? C18 H18B 0.9900 . ? C18 H18A 0.9900 . ? C19 C20 1.506(5) . ? C19 H19B 0.9900 . ? C19 H19A 0.9900 . ? C20 H20B 0.9900 . ? C20 H20A 0.9900 . ? C21 C22 1.514(5) . ? C21 H21B 0.9900 . ? C21 H21A 0.9900 . ? C22 H22B 0.9900 . ? C22 H22A 0.9900 . ? C23 C24 1.515(4) . ? C23 H23B 0.9900 . ? C23 H23A 0.9900 . ? C24 H24B 0.9900 . ? C24 H24A 0.9900 . ? C25 C26 1.499(4) . ? C26 C27 1.377(5) . ? C26 C31 1.389(5) . ? C27 C28 1.385(5) . ? C27 H27A 0.9500 . ? C28 C29 1.375(7) . ? C28 H28A 0.9500 . ? C29 C30 1.369(7) . ? C29 H29A 0.9500 . ? C30 C31 1.390(6) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C33 1.500(4) . ? C33 C34 1.378(5) . ? C33 C38 1.388(4) . ? C34 C35 1.383(5) . ? C34 H34A 0.9500 . ? C35 C36 1.372(5) . ? C35 H35A 0.9500 . ? C36 C37 1.372(5) . ? C36 H36A 0.9500 . ? C37 C38 1.387(5) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.508(4) . ? C40 C45 1.382(5) . ? C40 C41 1.386(5) . ? C41 C42 1.394(5) . ? C41 H41A 0.9500 . ? C42 C43 1.366(6) . ? C42 H42A 0.9500 . ? C43 C44 1.372(6) . ? C43 H43A 0.9500 . ? C44 C45 1.386(5) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 C47 1.481(5) . ? C47 C52 1.363(5) . ? C47 C48 1.398(5) . ? C48 C49 1.367(6) . ? C48 H48A 0.9500 . ? C49 C50 1.386(7) . ? C49 H49A 0.9500 . ? C50 C51 1.381(6) . ? C50 H50A 0.9500 . ? C51 C52 1.383(6) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 C54 1.502(4) . ? C54 C55 1.385(4) . ? C54 C59 1.394(5) . ? C55 C56 1.387(5) . ? C55 H55A 0.9500 . ? C56 C57 1.373(5) . ? C56 H56A 0.9500 . ? C57 C58 1.368(5) . ? C57 H57A 0.9500 . ? C58 C59 1.381(5) . ? C58 H58A 0.9500 . ? C59 H59A 0.9500 . ? C60 C61 1.498(4) . ? C61 C62 1.392(4) . ? C61 C66 1.396(4) . ? C62 C63 1.379(5) . ? C62 H62A 0.9500 . ? C63 C64 1.379(5) . ? C63 H63A 0.9500 . ? C64 C65 1.377(5) . ? C64 H64A 0.9500 . ? C65 C66 1.387(5) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C67 C68 1.494(5) . ? C68 C73 1.370(5) . ? C68 C69 1.403(5) . ? C69 C70 1.379(5) . ? C69 H69A 0.9500 . ? C70 C71 1.384(6) . ? C70 H70A 0.9500 . ? C71 C72 1.381(6) . ? C71 H71A 0.9500 . ? C72 C73 1.394(5) . ? C72 H72A 0.9500 . ? C73 H73A 0.9500 . ? C74 C75 1.500(4) . ? C75 C80 1.389(5) . ? C75 C76 1.395(5) . ? C76 C77 1.378(5) . ? C76 H76A 0.9500 . ? C77 C78 1.371(6) . ? C77 H77A 0.9500 . ? C78 C79 1.385(6) . ? C78 H78A 0.9500 . ? C79 C80 1.391(5) . ? C79 H79A 0.9500 . ? C80 H80A 0.9500 . ? C81 C82 1.504(4) . ? C82 C83 1.384(5) . ? C82 C87 1.385(4) . ? C83 C84 1.389(5) . ? C83 H83A 0.9500 . ? C84 C85 1.379(5) . ? C84 H84A 0.9500 . ? C85 C86 1.363(5) . ? C85 H85A 0.9500 . ? C86 C87 1.379(5) . ? C86 H86A 0.9500 . ? C87 H87A 0.9500 . ? C88 C89 1.411(8) . ? C89 H89C 0.9800 . ? C89 H89B 0.9800 . ? C89 H89A 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Fe1 O3 82.27(8) . . ? O4 Fe1 O5 102.68(9) . . ? O3 Fe1 O5 172.95(9) . . ? O4 Fe1 O1 99.17(8) . . ? O3 Fe1 O1 96.43(9) . . ? O5 Fe1 O1 87.79(9) . . ? O4 Fe1 O2 98.87(9) . . ? O3 Fe1 O2 88.35(9) . . ? O5 Fe1 O2 85.93(9) . . ? O1 Fe1 O2 161.80(9) . . ? O4 Fe1 N1 160.20(9) . . ? O3 Fe1 N1 78.26(9) . . ? O5 Fe1 N1 97.04(9) . . ? O1 Fe1 N1 79.57(9) . . ? O2 Fe1 N1 84.27(9) . . ? O3 Fe2 O6 95.08(9) . . ? O3 Fe2 O7 95.01(9) . . ? O6 Fe2 O7 96.96(9) . . ? O3 Fe2 O9 160.13(8) . . ? O6 Fe2 O9 80.35(8) . . ? O7 Fe2 O9 104.71(8) . . ? O3 Fe2 O8 101.83(9) . . ? O6 Fe2 O8 163.07(8) . . ? O7 Fe2 O8 80.76(8) . . ? O9 Fe2 O8 84.01(8) . . ? O3 Fe2 O4 79.20(8) . . ? O6 Fe2 O4 101.07(8) . . ? O7 Fe2 O4 161.46(8) . . ? O9 Fe2 O4 82.71(8) . . ? O8 Fe2 O4 83.21(8) . . ? O3 Fe2 Fe3 120.16(6) . . ? O6 Fe2 Fe3 120.63(6) . . ? O7 Fe2 Fe3 122.55(6) . . ? O9 Fe2 Fe3 49.96(6) . . ? O8 Fe2 Fe3 50.47(6) . . ? O4 Fe2 Fe3 49.94(5) . . ? O3 Fe2 Fe5 109.40(6) . . ? O6 Fe2 Fe5 131.48(6) . . ? O7 Fe2 Fe5 41.47(6) . . ? O9 Fe2 Fe5 87.51(6) . . ? O8 Fe2 Fe5 40.70(6) . . ? O4 Fe2 Fe5 123.82(6) . . ? Fe3 Fe2 Fe5 82.495(17) . . ? O3 Fe2 Fe7 128.31(7) . . ? O6 Fe2 Fe7 41.11(6) . . ? O7 Fe2 Fe7 112.58(6) . . ? O9 Fe2 Fe7 40.68(6) . . ? O8 Fe2 Fe7 124.40(6) . . ? O4 Fe2 Fe7 84.25(6) . . ? Fe3 Fe2 Fe7 81.119(16) . . ? Fe5 Fe2 Fe7 120.371(18) . . ? O10 Fe3 O11 112.33(9) . . ? O10 Fe3 O12 110.82(9) . . ? O11 Fe3 O12 111.11(9) . . ? O10 Fe3 O9 76.21(8) . . ? O11 Fe3 O9 150.27(8) . . ? O12 Fe3 O9 90.40(8) . . ? O10 Fe3 O4 150.78(8) . . ? O11 Fe3 O4 89.81(8) . . ? O12 Fe3 O4 75.91(8) . . ? O9 Fe3 O4 75.34(7) . . ? O10 Fe3 O8 90.71(8) . . ? O11 Fe3 O8 75.98(8) . . ? O12 Fe3 O8 150.87(8) . . ? O9 Fe3 O8 75.49(7) . . ? O4 Fe3 O8 75.90(7) . . ? O10 Fe3 Fe2 107.07(6) . . ? O11 Fe3 Fe2 107.42(6) . . ? O12 Fe3 Fe2 107.84(6) . . ? O9 Fe3 Fe2 44.36(5) . . ? O4 Fe3 Fe2 45.78(5) . . ? O8 Fe3 Fe2 44.97(5) . . ? O11 Fe4 O14 93.11(9) . . ? O11 Fe4 O8 82.09(8) . . ? O14 Fe4 O8 171.19(9) . . ? O11 Fe4 O1 88.98(9) . . ? O14 Fe4 O1 93.78(9) . . ? O8 Fe4 O1 93.51(8) . . ? O11 Fe4 O15 176.47(9) . . ? O14 Fe4 O15 88.07(9) . . ? O8 Fe4 O15 97.16(9) . . ? O1 Fe4 O15 87.63(9) . . ? O11 Fe4 O13 94.64(9) . . ? O14 Fe4 O13 82.54(9) . . ? O8 Fe4 O13 90.46(8) . . ? O1 Fe4 O13 174.96(9) . . ? O15 Fe4 O13 88.81(9) . . ? O8 Fe5 O18 96.89(8) . . ? O8 Fe5 O7 82.95(8) . . ? O18 Fe5 O7 96.82(9) . . ? O8 Fe5 O17 101.97(9) . . ? O18 Fe5 O17 88.72(9) . . ? O7 Fe5 O17 172.15(9) . . ? O8 Fe5 O16 100.43(9) . . ? O18 Fe5 O16 162.33(9) . . ? O7 Fe5 O16 88.78(9) . . ? O17 Fe5 O16 84.32(9) . . ? O8 Fe5 N2 160.64(9) . . ? O18 Fe5 N2 80.62(9) . . ? O7 Fe5 N2 78.33(9) . . ? O17 Fe5 N2 97.19(10) . . ? O16 Fe5 N2 84.16(9) . . ? O8 Fe5 Fe2 43.80(6) . . ? O18 Fe5 Fe2 90.51(6) . . ? O7 Fe5 Fe2 40.61(6) . . ? O17 Fe5 Fe2 145.34(7) . . ? O16 Fe5 Fe2 104.41(7) . . ? N2 Fe5 Fe2 116.85(7) . . ? O20 Fe6 O10 94.62(9) . . ? O20 Fe6 O18 92.59(9) . . ? O10 Fe6 O18 90.31(9) . . ? O20 Fe6 O9 170.96(9) . . ? O10 Fe6 O9 80.81(8) . . ? O18 Fe6 O9 95.21(8) . . ? O20 Fe6 O19 90.98(9) . . ? O10 Fe6 O19 173.48(9) . . ? O18 Fe6 O19 86.10(9) . . ? O9 Fe6 O19 94.09(8) . . ? O20 Fe6 O21 84.19(9) . . ? O10 Fe6 O21 91.10(9) . . ? O18 Fe6 O21 176.58(9) . . ? O9 Fe6 O21 88.09(8) . . ? O19 Fe6 O21 92.79(9) . . ? O9 Fe7 O6 81.60(8) . . ? O9 Fe7 O24 100.78(8) . . ? O6 Fe7 O24 95.29(9) . . ? O9 Fe7 O23 101.15(9) . . ? O6 Fe7 O23 175.65(9) . . ? O24 Fe7 O23 87.53(9) . . ? O9 Fe7 O22 98.92(8) . . ? O6 Fe7 O22 86.61(9) . . ? O24 Fe7 O22 160.28(8) . . ? O23 Fe7 O22 89.62(9) . . ? O9 Fe7 N3 160.54(9) . . ? O6 Fe7 N3 78.97(9) . . ? O24 Fe7 N3 79.88(9) . . ? O23 Fe7 N3 98.31(9) . . ? O22 Fe7 N3 81.23(9) . . ? O9 Fe7 Fe2 42.95(6) . . ? O6 Fe7 Fe2 40.13(6) . . ? O24 Fe7 Fe2 91.96(6) . . ? O23 Fe7 Fe2 143.26(7) . . ? O22 Fe7 Fe2 101.85(6) . . ? N3 Fe7 Fe2 117.77(7) . . ? O12 Fe8 O4 81.45(8) . . ? O12 Fe8 O24 91.55(8) . . ? O4 Fe8 O24 93.97(8) . . ? O12 Fe8 O25 93.57(9) . . ? O4 Fe8 O25 172.91(9) . . ? O24 Fe8 O25 91.20(8) . . ? O12 Fe8 O26 178.52(10) . . ? O4 Fe8 O26 97.99(8) . . ? O24 Fe8 O26 87.12(9) . . ? O25 Fe8 O26 87.11(9) . . ? O12 Fe8 O27 94.08(9) . . ? O4 Fe8 O27 89.31(8) . . ? O24 Fe8 O27 173.85(9) . . ? O25 Fe8 O27 86.01(9) . . ? O26 Fe8 O27 87.27(9) . . ? C2 O1 Fe4 119.77(19) . . ? C2 O1 Fe1 111.41(18) . . ? Fe4 O1 Fe1 128.37(11) . . ? C32 O2 Fe1 128.5(2) . . ? C4 O3 Fe2 133.61(19) . . ? C4 O3 Fe1 121.10(19) . . ? Fe2 O3 Fe1 99.68(9) . . ? Fe1 O4 Fe8 115.46(10) . . ? Fe1 O4 Fe2 95.65(8) . . ? Fe8 O4 Fe2 134.82(10) . . ? Fe1 O4 Fe3 132.75(10) . . ? Fe8 O4 Fe3 95.78(8) . . ? Fe2 O4 Fe3 84.28(7) . . ? C25 O5 Fe1 125.5(2) . . ? C16 O6 Fe2 136.74(19) . . ? C16 O6 Fe7 120.00(18) . . ? Fe2 O6 Fe7 98.76(9) . . ? C12 O7 Fe2 137.02(19) . . ? C12 O7 Fe5 120.83(18) . . ? Fe2 O7 Fe5 97.91(9) . . ? Fe5 O8 Fe4 114.62(10) . . ? Fe5 O8 Fe2 95.50(8) . . ? Fe4 O8 Fe2 135.85(10) . . ? Fe5 O8 Fe3 134.61(10) . . ? Fe4 O8 Fe3 94.71(8) . . ? Fe2 O8 Fe3 84.56(7) . . ? Fe7 O9 Fe6 116.51(10) . . ? Fe7 O9 Fe2 96.37(8) . . ? Fe6 O9 Fe2 131.90(10) . . ? Fe7 O9 Fe3 132.10(10) . . ? Fe6 O9 Fe3 95.39(8) . . ? Fe2 O9 Fe3 85.67(7) . . ? C22 O10 Fe3 121.96(18) . . ? C22 O10 Fe6 130.44(19) . . ? Fe3 O10 Fe6 107.56(9) . . ? C20 O11 Fe3 121.56(19) . . ? C20 O11 Fe4 130.86(19) . . ? Fe3 O11 Fe4 107.12(10) . . ? C24 O12 Fe3 120.85(18) . . ? C24 O12 Fe8 131.91(18) . . ? Fe3 O12 Fe8 106.83(9) . . ? C74 O13 Fe4 132.3(2) . . ? C67 O14 Fe4 136.7(2) . . ? C39 O15 Fe4 137.5(2) . . ? C39 O16 Fe5 125.4(2) . . ? C74 O17 Fe5 128.7(2) . . ? C10 O18 Fe5 111.28(18) . . ? C10 O18 Fe6 117.49(18) . . ? Fe5 O18 Fe6 130.10(11) . . ? C60 O19 Fe6 137.3(2) . . ? C46 O20 Fe6 136.8(2) . . ? C53 O21 Fe6 137.8(2) . . ? C60 O22 Fe7 129.5(2) . . ? C53 O23 Fe7 124.5(2) . . ? C14 O24 Fe8 121.17(18) . . ? C14 O24 Fe7 111.61(17) . . ? Fe8 O24 Fe7 127.17(10) . . ? C81 O25 Fe8 138.4(2) . . ? C32 O26 Fe8 136.3(2) . . ? C25 O27 Fe8 135.9(2) . . ? C18 O31 H31 109.5 . . ? C6 O32 H32 109.5 . . ? C8 O33 H33 109.5 . . ? C3 N1 C5 112.0(2) . . ? C3 N1 C1 111.3(3) . . ? C5 N1 C1 110.6(3) . . ? C3 N1 Fe1 104.21(18) . . ? C5 N1 Fe1 112.81(19) . . ? C1 N1 Fe1 105.56(19) . . ? C11 N2 C9 111.6(3) . . ? C11 N2 C7 112.4(3) . . ? C9 N2 C7 112.3(3) . . ? C11 N2 Fe5 104.89(19) . . ? C9 N2 Fe5 104.85(18) . . ? C7 N2 Fe5 110.23(19) . . ? C15 N3 C13 111.2(2) . . ? C15 N3 C17 113.8(2) . . ? C13 N3 C17 111.4(2) . . ? C15 N3 Fe7 103.46(18) . . ? C13 N3 Fe7 105.85(18) . . ? C17 N3 Fe7 110.60(19) . . ? C23 N4 C21 114.0(3) . . ? C23 N4 C19 113.7(3) . . ? C21 N4 C19 113.3(3) . . ? N1 C1 C2 109.3(3) . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? H1B C1 H1A 108.3 . . ? O1 C2 C1 108.0(3) . . ? O1 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? O1 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? H2B C2 H2A 108.4 . . ? N1 C3 C4 110.4(3) . . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? H3B C3 H3A 108.1 . . ? O3 C4 C3 107.3(3) . . ? O3 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? O3 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? H4B C4 H4A 108.5 . . ? N1 C5 C6 115.3(3) . . ? N1 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? N1 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? H5B C5 H5A 107.5 . . ? O32 C6 C5 110.9(3) . . ? O32 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? O32 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? H6B C6 H6A 108.0 . . ? N2 C7 C8 117.2(3) . . ? N2 C7 H7B 108.0 . . ? C8 C7 H7B 108.0 . . ? N2 C7 H7A 108.0 . . ? C8 C7 H7A 108.0 . . ? H7B C7 H7A 107.2 . . ? O33 C8 C7 107.6(3) . . ? O33 C8 H8B 110.2 . . ? C7 C8 H8B 110.2 . . ? O33 C8 H8A 110.2 . . ? C7 C8 H8A 110.2 . . ? H8B C8 H8A 108.5 . . ? N2 C9 C10 109.0(3) . . ? N2 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? N2 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? H9B C9 H9A 108.3 . . ? O18 C10 C9 107.2(3) . . ? O18 C10 H10B 110.3 . . ? C9 C10 H10B 110.3 . . ? O18 C10 H10A 110.3 . . ? C9 C10 H10A 110.3 . . ? H10B C10 H10A 108.5 . . ? N2 C11 C12 109.9(3) . . ? N2 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? N2 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? H11B C11 H11A 108.2 . . ? O7 C12 C11 108.0(3) . . ? O7 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? O7 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? H12B C12 H12A 108.4 . . ? N3 C13 C14 109.4(2) . . ? N3 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? N3 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? H13B C13 H13A 108.2 . . ? O24 C14 C13 108.0(2) . . ? O24 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? O24 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? H14B C14 H14A 108.4 . . ? N3 C15 C16 110.4(3) . . ? N3 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? N3 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? H15B C15 H15A 108.1 . . ? O6 C16 C15 107.4(3) . . ? O6 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? O6 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? H16B C16 H16A 108.5 . . ? N3 C17 C18 118.3(3) . . ? N3 C17 H17B 107.7 . . ? C18 C17 H17B 107.7 . . ? N3 C17 H17A 107.7 . . ? C18 C17 H17A 107.7 . . ? H17B C17 H17A 107.1 . . ? O31 C18 C17 113.9(3) . . ? O31 C18 H18B 108.8 . . ? C17 C18 H18B 108.8 . . ? O31 C18 H18A 108.8 . . ? C17 C18 H18A 108.8 . . ? H18B C18 H18A 107.7 . . ? N4 C19 C20 107.6(3) . . ? N4 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? N4 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? H19B C19 H19A 108.5 . . ? O11 C20 C19 106.3(3) . . ? O11 C20 H20B 110.5 . . ? C19 C20 H20B 110.5 . . ? O11 C20 H20A 110.5 . . ? C19 C20 H20A 110.5 . . ? H20B C20 H20A 108.7 . . ? N4 C21 C22 108.6(3) . . ? N4 C21 H21B 110.0 . . ? C22 C21 H21B 110.0 . . ? N4 C21 H21A 110.0 . . ? C22 C21 H21A 110.0 . . ? H21B C21 H21A 108.4 . . ? O10 C22 C21 107.5(3) . . ? O10 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? O10 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? H22B C22 H22A 108.5 . . ? N4 C23 C24 107.9(2) . . ? N4 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? N4 C23 H23A 110.1 . . ? C24 C23 H23A 110.1 . . ? H23B C23 H23A 108.4 . . ? O12 C24 C23 107.1(2) . . ? O12 C24 H24B 110.3 . . ? C23 C24 H24B 110.3 . . ? O12 C24 H24A 110.3 . . ? C23 C24 H24A 110.3 . . ? H24B C24 H24A 108.5 . . ? O27 C25 O5 125.2(3) . . ? O27 C25 C26 117.5(3) . . ? O5 C25 C26 117.3(3) . . ? C27 C26 C31 119.6(4) . . ? C27 C26 C25 119.5(3) . . ? C31 C26 C25 120.9(3) . . ? C26 C27 C28 120.6(4) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C29 C28 C27 119.6(5) . . ? C29 C28 H28A 120.2 . . ? C27 C28 H28A 120.2 . . ? C30 C29 C28 120.4(4) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 120.3(4) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C26 C31 C30 119.5(4) . . ? C26 C31 H31A 120.3 . . ? C30 C31 H31A 120.3 . . ? O2 C32 O26 124.6(3) . . ? O2 C32 C33 118.7(3) . . ? O26 C32 C33 116.7(3) . . ? C34 C33 C38 119.1(3) . . ? C34 C33 C32 119.9(3) . . ? C38 C33 C32 120.9(3) . . ? C33 C34 C35 120.8(4) . . ? C33 C34 H34A 119.6 . . ? C35 C34 H34A 119.6 . . ? C36 C35 C34 119.9(4) . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C37 C36 C35 119.8(3) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C36 C37 C38 120.8(4) . . ? C36 C37 H37A 119.6 . . ? C38 C37 H37A 119.6 . . ? C37 C38 C33 119.5(3) . . ? C37 C38 H38A 120.2 . . ? C33 C38 H38A 120.2 . . ? O15 C39 O16 125.7(3) . . ? O15 C39 C40 116.4(3) . . ? O16 C39 C40 117.9(3) . . ? C45 C40 C41 119.0(3) . . ? C45 C40 C39 120.6(3) . . ? C41 C40 C39 120.3(3) . . ? C40 C41 C42 120.1(3) . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C43 C42 C41 119.8(4) . . ? C43 C42 H42A 120.1 . . ? C41 C42 H42A 120.1 . . ? C42 C43 C44 120.8(4) . . ? C42 C43 H43A 119.6 . . ? C44 C43 H43A 119.6 . . ? C43 C44 C45 119.6(4) . . ? C43 C44 H44A 120.2 . . ? C45 C44 H44A 120.2 . . ? C40 C45 C44 120.7(4) . . ? C40 C45 H45A 119.7 . . ? C44 C45 H45A 119.7 . . ? O29 C46 O20 122.3(3) . . ? O29 C46 C47 119.4(3) . . ? O20 C46 C47 118.3(3) . . ? C52 C47 C48 119.2(4) . . ? C52 C47 C46 121.5(3) . . ? C48 C47 C46 119.3(3) . . ? C49 C48 C47 119.7(4) . . ? C49 C48 H48A 120.1 . . ? C47 C48 H48A 120.1 . . ? C48 C49 C50 120.9(4) . . ? C48 C49 H49A 119.6 . . ? C50 C49 H49A 119.6 . . ? C51 C50 C49 119.3(4) . . ? C51 C50 H50A 120.4 . . ? C49 C50 H50A 120.4 . . ? C50 C51 C52 119.6(5) . . ? C50 C51 H51A 120.2 . . ? C52 C51 H51A 120.2 . . ? C47 C52 C51 121.3(4) . . ? C47 C52 H52A 119.4 . . ? C51 C52 H52A 119.4 . . ? O21 C53 O23 125.4(3) . . ? O21 C53 C54 116.9(3) . . ? O23 C53 C54 117.7(3) . . ? C55 C54 C59 119.4(3) . . ? C55 C54 C53 120.7(3) . . ? C59 C54 C53 119.6(3) . . ? C54 C55 C56 119.7(3) . . ? C54 C55 H55A 120.1 . . ? C56 C55 H55A 120.1 . . ? C57 C56 C55 120.5(4) . . ? C57 C56 H56A 119.8 . . ? C55 C56 H56A 119.8 . . ? C58 C57 C56 120.0(3) . . ? C58 C57 H57A 120.0 . . ? C56 C57 H57A 120.0 . . ? C57 C58 C59 120.6(4) . . ? C57 C58 H58A 119.7 . . ? C59 C58 H58A 119.7 . . ? C58 C59 C54 119.8(3) . . ? C58 C59 H59A 120.1 . . ? C54 C59 H59A 120.1 . . ? O22 C60 O19 125.1(3) . . ? O22 C60 C61 117.4(3) . . ? O19 C60 C61 117.6(3) . . ? C62 C61 C66 119.5(3) . . ? C62 C61 C60 120.3(3) . . ? C66 C61 C60 120.2(3) . . ? C63 C62 C61 119.9(3) . . ? C63 C62 H62A 120.1 . . ? C61 C62 H62A 120.1 . . ? C62 C63 C64 120.5(4) . . ? C62 C63 H63A 119.8 . . ? C64 C63 H63A 119.8 . . ? C65 C64 C63 120.2(3) . . ? C65 C64 H64A 119.9 . . ? C63 C64 H64A 119.9 . . ? C64 C65 C66 120.2(4) . . ? C64 C65 H65A 119.9 . . ? C66 C65 H65A 119.9 . . ? C65 C66 C61 119.7(3) . . ? C65 C66 H66A 120.1 . . ? C61 C66 H66A 120.1 . . ? O28 C67 O14 123.9(3) . . ? O28 C67 C68 119.3(3) . . ? O14 C67 C68 116.7(3) . . ? C73 C68 C69 119.3(4) . . ? C73 C68 C67 120.7(3) . . ? C69 C68 C67 119.9(3) . . ? C70 C69 C68 119.9(4) . . ? C70 C69 H69A 120.1 . . ? C68 C69 H69A 120.1 . . ? C69 C70 C71 120.5(4) . . ? C69 C70 H70A 119.8 . . ? C71 C70 H70A 119.8 . . ? C72 C71 C70 119.8(4) . . ? C72 C71 H71A 120.1 . . ? C70 C71 H71A 120.1 . . ? C71 C72 C73 119.8(4) . . ? C71 C72 H72A 120.1 . . ? C73 C72 H72A 120.1 . . ? C68 C73 C72 120.7(4) . . ? C68 C73 H73A 119.6 . . ? C72 C73 H73A 119.6 . . ? O13 C74 O17 124.7(3) . . ? O13 C74 C75 118.9(3) . . ? O17 C74 C75 116.3(3) . . ? C80 C75 C76 119.4(3) . . ? C80 C75 C74 120.5(3) . . ? C76 C75 C74 120.1(3) . . ? C77 C76 C75 120.4(4) . . ? C77 C76 H76A 119.8 . . ? C75 C76 H76A 119.8 . . ? C78 C77 C76 120.3(4) . . ? C78 C77 H77A 119.8 . . ? C76 C77 H77A 119.8 . . ? C77 C78 C79 119.9(4) . . ? C77 C78 H78A 120.1 . . ? C79 C78 H78A 120.1 . . ? C78 C79 C80 120.5(4) . . ? C78 C79 H79A 119.7 . . ? C80 C79 H79A 119.7 . . ? C75 C80 C79 119.4(4) . . ? C75 C80 H80A 120.3 . . ? C79 C80 H80A 120.3 . . ? O30 C81 O25 124.8(3) . . ? O30 C81 C82 119.7(3) . . ? O25 C81 C82 115.6(3) . . ? C83 C82 C87 118.5(3) . . ? C83 C82 C81 120.3(3) . . ? C87 C82 C81 121.1(3) . . ? C82 C83 C84 120.1(3) . . ? C82 C83 H83A 119.9 . . ? C84 C83 H83A 119.9 . . ? C85 C84 C83 120.2(4) . . ? C85 C84 H84A 119.9 . . ? C83 C84 H84A 119.9 . . ? C86 C85 C84 120.0(4) . . ? C86 C85 H85A 120.0 . . ? C84 C85 H85A 120.0 . . ? C85 C86 C87 120.1(3) . . ? C85 C86 H86A 120.0 . . ? C87 C86 H86A 120.0 . . ? C86 C87 C82 121.1(3) . . ? C86 C87 H87A 119.4 . . ? C82 C87 H87A 119.4 . . ? N5 C88 C89 176.6(8) . . ? C88 C89 H89C 109.5 . . ? C88 C89 H89B 109.5 . . ? H89C C89 H89B 109.5 . . ? C88 C89 H89A 109.5 . . ? H89C C89 H89A 109.5 . . ? H89B C89 H89A 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O31 H31 O28 0.84 1.98 2.795(4) 162.9 2_655 O32 H32 O30 0.84 1.87 2.700(3) 171.0 4_545 O33 H33 O32 0.84 1.91 2.731(4) 163.6 4_546 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.643 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.068 #===END data_xm40 _database_code_CSD 217873 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H84 Fe6 N6 O32' _chemical_formula_weight 1496.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 11.5538(6) _cell_length_b 11.5495(6) _cell_length_c 22.3761(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.724(2) _cell_angle_gamma 90.00 _cell_volume 2887.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 163 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7383 _exptl_absorpt_correction_T_max 0.7975 _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 24572 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6547 _reflns_number_gt 5498 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+1.7625P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6547 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.12040(3) 0.77675(3) -0.037261(14) 0.02107(8) Uani 1 1 d . . . Fe2 Fe 0.25881(3) 0.93492(3) 0.070078(14) 0.02114(8) Uani 1 1 d . . . Fe3 Fe 0.13988(3) 1.15562(3) 0.108316(14) 0.01954(8) Uani 1 1 d . . . O1 O 0.2236(4) 0.4560(2) -0.06995(14) 0.1050(13) Uani 1 1 d . . . O2 O 0.18565(15) 0.61664(15) -0.02324(7) 0.0315(4) Uani 1 1 d . . . O3 O 0.02725(13) 0.89665(13) -0.09475(7) 0.0241(3) Uani 1 1 d . . . O4 O 0.27256(13) 0.86656(14) -0.00827(7) 0.0261(3) Uani 1 1 d . . . O5 O 0.11906(14) 0.82500(14) 0.04711(7) 0.0252(3) Uani 1 1 d . . . O6 O 0.61321(18) 0.8836(2) 0.13301(14) 0.0747(8) Uani 1 1 d . . . O7 O 0.43422(14) 0.96550(15) 0.09589(8) 0.0318(4) Uani 1 1 d . . . O8 O 0.19319(13) 1.08580(13) 0.03778(7) 0.0232(3) Uani 1 1 d . . . O9 O 0.21443(14) 1.00829(14) 0.14216(7) 0.0263(3) Uani 1 1 d . . . O10 O 0.04360(13) 1.28603(13) 0.06213(7) 0.0250(3) Uani 1 1 d . . . O11 O 0.18544(14) 1.22471(14) 0.19228(7) 0.0273(3) Uani 1 1 d . . . O12 O 0.3314(2) 1.3073(2) 0.26383(9) 0.0551(6) Uani 1 1 d . . . N1 N 0.19995(17) 0.75503(17) -0.11625(9) 0.0269(4) Uani 1 1 d . . . N2 N 0.31973(18) 0.80214(17) 0.14164(9) 0.0280(4) Uani 1 1 d . . . N3 N 0.28227(16) 1.27880(16) 0.10082(8) 0.0227(4) Uani 1 1 d . . . C1 C 0.1893(3) 0.6294(2) -0.12934(14) 0.0517(8) Uani 1 1 d . . . H1A H 0.2520 0.6052 -0.1498 0.062 Uiso 1 1 calc R . . H1B H 0.1103 0.6129 -0.1579 0.062 Uiso 1 1 calc R . . C2 C 0.2024(3) 0.5608(3) -0.07011(15) 0.0545(9) Uani 1 1 d . . . C3 C 0.1288(3) 0.8253(3) -0.16808(11) 0.0381(6) Uani 1 1 d . . . H3A H 0.0617 0.7785 -0.1928 0.046 Uiso 1 1 calc R . . H3B H 0.1797 0.8492 -0.1954 0.046 Uiso 1 1 calc R . . C4 C 0.0798(2) 0.9321(2) -0.14285(13) 0.0379(6) Uani 1 1 d . . . H4B H 0.1454 0.9878 -0.1266 0.045 Uiso 1 1 calc R . . H4A H 0.0191 0.9705 -0.1762 0.045 Uiso 1 1 calc R . . C5 C 0.3257(3) 0.7881(4) -0.09517(14) 0.0605(10) Uani 1 1 d . . . H5A H 0.3736 0.7175 -0.0813 0.073 Uiso 1 1 calc R . . H5B H 0.3515 0.8201 -0.1308 0.073 Uiso 1 1 calc R . . C6 C 0.3528(3) 0.8711(3) -0.04606(16) 0.0575(10) Uani 1 1 d . . . H6A H 0.4349 0.8570 -0.0204 0.069 Uiso 1 1 calc R . . H6B H 0.3508 0.9497 -0.0639 0.069 Uiso 1 1 calc R . . C7 C 0.3240(3) 0.8565(2) 0.20194(11) 0.0398(6) Uani 1 1 d . . . H7A H 0.3132 0.7959 0.2313 0.048 Uiso 1 1 calc R . . H7B H 0.4040 0.8915 0.2184 0.048 Uiso 1 1 calc R . . C8 C 0.2319(3) 0.9466(3) 0.19838(12) 0.0491(8) Uani 1 1 d . . . H8A H 0.1557 0.9103 0.2009 0.059 Uiso 1 1 calc R . . H8B H 0.2575 1.0007 0.2336 0.059 Uiso 1 1 calc R . . C9 C 0.4418(2) 0.7739(2) 0.13690(14) 0.0424(7) Uani 1 1 d . . . H9A H 0.4376 0.7154 0.1041 0.051 Uiso 1 1 calc R . . H9B H 0.4886 0.7407 0.1765 0.051 Uiso 1 1 calc R . . C10 C 0.5035(2) 0.8819(3) 0.12192(14) 0.0432(7) Uani 1 1 d . . . C11 C 0.2353(3) 0.7031(2) 0.12681(12) 0.0379(6) Uani 1 1 d . . . H11A H 0.2335 0.6616 0.1653 0.045 Uiso 1 1 calc R . . H11B H 0.2628 0.6482 0.0993 0.045 Uiso 1 1 calc R . . C12 C 0.1105(2) 0.7463(2) 0.09515(11) 0.0371(6) Uani 1 1 d . . . H12A H 0.0584 0.6802 0.0775 0.045 Uiso 1 1 calc R . . H12B H 0.0750 0.7859 0.1255 0.045 Uiso 1 1 calc R . . C13 C 0.3639(2) 1.2777(2) 0.16349(11) 0.0334(5) Uani 1 1 d . . . H13A H 0.4134 1.3488 0.1702 0.040 Uiso 1 1 calc R . . H13B H 0.4181 1.2100 0.1681 0.040 Uiso 1 1 calc R . . C14 C 0.2893(2) 1.2713(2) 0.21108(11) 0.0333(5) Uani 1 1 d . . . C15 C 0.2243(2) 1.3943(2) 0.08840(12) 0.0301(5) Uani 1 1 d . . . H15A H 0.2745 1.4457 0.0700 0.036 Uiso 1 1 calc R . . H15B H 0.2180 1.4294 0.1278 0.036 Uiso 1 1 calc R . . C16 C 0.1020(2) 1.3847(2) 0.04531(12) 0.0320(5) Uani 1 1 d . . . H16A H 0.0551 1.4554 0.0480 0.038 Uiso 1 1 calc R . . H16B H 0.1085 1.3767 0.0022 0.038 Uiso 1 1 calc R . . C17 C 0.3381(2) 1.2375(2) 0.05189(11) 0.0317(5) Uani 1 1 d . . . H17A H 0.4094 1.1900 0.0706 0.038 Uiso 1 1 calc R . . H17B H 0.3642 1.3046 0.0311 0.038 Uiso 1 1 calc R . . C18 C 0.2479(2) 1.1653(2) 0.00470(11) 0.0301(5) Uani 1 1 d . . . H18A H 0.1865 1.2163 -0.0214 0.036 Uiso 1 1 calc R . . H18B H 0.2891 1.1229 -0.0224 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01804(15) 0.02562(17) 0.01966(15) -0.00078(12) 0.00501(12) 0.00274(12) Fe2 0.02081(16) 0.02107(16) 0.02046(15) -0.00023(12) 0.00327(12) 0.00327(12) Fe3 0.01876(15) 0.01958(16) 0.01962(15) -0.00009(12) 0.00367(11) 0.00190(11) O1 0.209(4) 0.0471(15) 0.097(2) 0.0309(14) 0.109(3) 0.061(2) O2 0.0321(9) 0.0368(9) 0.0288(8) 0.0081(7) 0.0134(7) 0.0143(7) O3 0.0214(7) 0.0237(8) 0.0277(8) 0.0018(6) 0.0073(6) 0.0007(6) O4 0.0200(7) 0.0340(9) 0.0266(8) -0.0046(7) 0.0101(6) -0.0009(6) O5 0.0251(8) 0.0307(9) 0.0210(7) -0.0018(6) 0.0078(6) -0.0024(6) O6 0.0264(11) 0.0848(18) 0.108(2) 0.0422(17) 0.0087(12) 0.0120(11) O7 0.0225(8) 0.0341(9) 0.0355(9) 0.0036(7) 0.0011(7) 0.0008(7) O8 0.0267(8) 0.0225(8) 0.0197(7) 0.0009(6) 0.0046(6) 0.0042(6) O9 0.0335(8) 0.0250(8) 0.0199(7) 0.0030(6) 0.0059(6) 0.0093(7) O10 0.0219(7) 0.0201(7) 0.0310(8) 0.0030(6) 0.0028(6) 0.0010(6) O11 0.0302(8) 0.0305(9) 0.0222(8) -0.0043(7) 0.0086(6) -0.0017(7) O12 0.0645(14) 0.0735(15) 0.0248(9) -0.0140(10) 0.0067(9) -0.0266(12) N1 0.0285(10) 0.0302(10) 0.0229(9) 0.0005(8) 0.0080(8) 0.0049(8) N2 0.0316(10) 0.0259(10) 0.0253(10) 0.0010(8) 0.0048(8) 0.0035(8) N3 0.0215(9) 0.0239(9) 0.0223(9) -0.0001(7) 0.0046(7) 0.0004(7) C1 0.094(3) 0.0318(14) 0.0396(15) 0.0032(12) 0.0366(16) 0.0146(15) C2 0.084(2) 0.0397(17) 0.0539(18) 0.0119(14) 0.0423(17) 0.0272(16) C3 0.0443(15) 0.0475(16) 0.0266(12) 0.0120(11) 0.0163(11) 0.0124(12) C4 0.0373(14) 0.0350(14) 0.0476(15) 0.0165(12) 0.0221(12) 0.0076(11) C5 0.0290(14) 0.115(3) 0.0429(16) -0.0283(19) 0.0198(13) -0.0110(17) C6 0.0389(16) 0.084(2) 0.0614(19) -0.0385(18) 0.0353(15) -0.0264(16) C7 0.0538(17) 0.0354(14) 0.0234(12) 0.0002(10) -0.0029(11) 0.0123(12) C8 0.079(2) 0.0445(17) 0.0248(12) 0.0078(12) 0.0140(13) 0.0270(16) C9 0.0390(15) 0.0369(15) 0.0504(17) 0.0111(13) 0.0094(13) 0.0174(12) C10 0.0271(13) 0.0489(17) 0.0504(16) 0.0117(14) 0.0038(12) 0.0112(12) C11 0.0540(16) 0.0267(13) 0.0302(13) 0.0034(10) 0.0055(12) -0.0069(11) C12 0.0427(15) 0.0444(15) 0.0252(12) 0.0003(11) 0.0105(11) -0.0161(12) C13 0.0253(12) 0.0452(15) 0.0262(12) -0.0002(11) 0.0003(9) -0.0061(10) C14 0.0382(14) 0.0381(14) 0.0220(11) -0.0025(10) 0.0048(10) -0.0048(11) C15 0.0284(12) 0.0214(11) 0.0387(13) 0.0010(10) 0.0050(10) -0.0019(9) C16 0.0304(12) 0.0213(11) 0.0431(14) 0.0069(10) 0.0069(11) -0.0001(9) C17 0.0361(13) 0.0315(13) 0.0327(12) 0.0017(10) 0.0183(11) -0.0019(10) C18 0.0426(14) 0.0276(12) 0.0226(11) 0.0018(9) 0.0129(10) 0.0032(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O10 1.9722(15) 3_575 ? Fe1 O5 1.9724(15) . ? Fe1 O2 1.9915(17) . ? Fe1 O4 2.0020(16) . ? Fe1 O3 2.0067(15) . ? Fe1 N1 2.2039(19) . ? Fe2 O8 1.9634(15) . ? Fe2 O4 1.9657(15) . ? Fe2 O7 1.9926(16) . ? Fe2 O9 2.0007(15) . ? Fe2 O5 2.0152(16) . ? Fe2 N2 2.1996(19) . ? Fe3 O9 1.9695(15) . ? Fe3 O3 1.9716(15) 3_575 ? Fe3 O11 1.9853(16) . ? Fe3 O10 1.9974(15) . ? Fe3 O8 2.0037(15) . ? Fe3 N3 2.2134(18) . ? O1 C2 1.235(4) . ? O2 C2 1.287(3) . ? O3 C4 1.424(3) . ? O3 Fe3 1.9716(15) 3_575 ? O4 C6 1.405(3) . ? O5 C12 1.431(3) . ? O6 C10 1.229(3) . ? O7 C10 1.294(3) . ? O8 C18 1.425(3) . ? O9 C8 1.415(3) . ? O10 C16 1.423(3) . ? O10 Fe1 1.9722(15) 3_575 ? O11 C14 1.284(3) . ? O12 C14 1.229(3) . ? N1 C5 1.460(3) . ? N1 C1 1.479(3) . ? N1 C3 1.482(3) . ? N2 C9 1.477(3) . ? N2 C7 1.478(3) . ? N2 C11 1.485(3) . ? N3 C13 1.478(3) . ? N3 C17 1.484(3) . ? N3 C15 1.487(3) . ? C1 C2 1.518(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.524(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C5 C6 1.432(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.476(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.516(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.521(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.533(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.499(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.528(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Fe1 O5 97.66(7) 3_575 . ? O10 Fe1 O2 90.07(7) 3_575 . ? O5 Fe1 O2 101.91(7) . . ? O10 Fe1 O4 169.58(7) 3_575 . ? O5 Fe1 O4 76.31(6) . . ? O2 Fe1 O4 99.44(7) . . ? O10 Fe1 O3 75.67(6) 3_575 . ? O5 Fe1 O3 106.57(7) . . ? O2 Fe1 O3 149.50(7) . . ? O4 Fe1 O3 97.69(7) . . ? O10 Fe1 N1 107.36(7) 3_575 . ? O5 Fe1 N1 154.98(7) . . ? O2 Fe1 N1 78.60(7) . . ? O4 Fe1 N1 78.93(7) . . ? O3 Fe1 N1 80.18(7) . . ? O8 Fe2 O4 98.01(7) . . ? O8 Fe2 O7 102.62(7) . . ? O4 Fe2 O7 91.31(7) . . ? O8 Fe2 O9 76.51(6) . . ? O4 Fe2 O9 169.90(6) . . ? O7 Fe2 O9 98.13(7) . . ? O8 Fe2 O5 104.82(7) . . ? O4 Fe2 O5 76.16(6) . . ? O7 Fe2 O5 151.11(7) . . ? O9 Fe2 O5 96.86(7) . . ? O8 Fe2 N2 155.35(7) . . ? O4 Fe2 N2 106.61(7) . . ? O7 Fe2 N2 78.40(7) . . ? O9 Fe2 N2 78.97(7) . . ? O5 Fe2 N2 80.44(7) . . ? O9 Fe3 O3 96.33(7) . 3_575 ? O9 Fe3 O11 89.92(7) . . ? O3 Fe3 O11 106.41(7) 3_575 . ? O9 Fe3 O10 169.12(7) . . ? O3 Fe3 O10 75.90(6) 3_575 . ? O11 Fe3 O10 99.52(7) . . ? O9 Fe3 O8 76.30(6) . . ? O3 Fe3 O8 103.92(6) 3_575 . ? O11 Fe3 O8 147.84(7) . . ? O10 Fe3 O8 97.95(6) . . ? O9 Fe3 N3 108.88(7) . . ? O3 Fe3 N3 154.54(7) 3_575 . ? O11 Fe3 N3 77.88(7) . . ? O10 Fe3 N3 78.64(6) . . ? O8 Fe3 N3 79.38(7) . . ? C2 O2 Fe1 117.77(17) . . ? C4 O3 Fe3 124.13(15) . 3_575 ? C4 O3 Fe1 114.86(14) . . ? Fe3 O3 Fe1 103.42(7) 3_575 . ? C6 O4 Fe2 137.46(16) . . ? C6 O4 Fe1 118.91(15) . . ? Fe2 O4 Fe1 103.51(7) . . ? C12 O5 Fe1 123.95(15) . . ? C12 O5 Fe2 114.40(14) . . ? Fe1 O5 Fe2 102.79(7) . . ? C10 O7 Fe2 117.72(17) . . ? C18 O8 Fe2 125.64(14) . . ? C18 O8 Fe3 114.56(13) . . ? Fe2 O8 Fe3 103.56(7) . . ? C8 O9 Fe3 136.59(15) . . ? C8 O9 Fe2 119.72(15) . . ? Fe3 O9 Fe2 103.45(7) . . ? C16 O10 Fe1 134.89(14) . 3_575 ? C16 O10 Fe3 120.12(13) . . ? Fe1 O10 Fe3 103.74(7) 3_575 . ? C14 O11 Fe3 118.63(15) . . ? C5 N1 C1 110.3(3) . . ? C5 N1 C3 114.7(2) . . ? C1 N1 C3 112.4(2) . . ? C5 N1 Fe1 107.15(15) . . ? C1 N1 Fe1 103.86(15) . . ? C3 N1 Fe1 107.68(14) . . ? C9 N2 C7 110.4(2) . . ? C9 N2 C11 113.5(2) . . ? C7 N2 C11 113.5(2) . . ? C9 N2 Fe2 103.67(15) . . ? C7 N2 Fe2 107.37(15) . . ? C11 N2 Fe2 107.70(14) . . ? C13 N3 C17 113.90(19) . . ? C13 N3 C15 109.49(19) . . ? C17 N3 C15 114.22(18) . . ? C13 N3 Fe3 103.29(14) . . ? C17 N3 Fe3 108.68(14) . . ? C15 N3 Fe3 106.42(13) . . ? N1 C1 C2 110.7(2) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? O1 C2 O2 124.0(3) . . ? O1 C2 C1 119.3(3) . . ? O2 C2 C1 116.6(2) . . ? N1 C3 C4 109.7(2) . . ? N1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O3 C4 C3 108.5(2) . . ? O3 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? O3 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? H4B C4 H4A 108.4 . . ? C6 C5 N1 115.4(2) . . ? C6 C5 H5A 108.4 . . ? N1 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? N1 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? O4 C6 C5 112.8(2) . . ? O4 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? O4 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 N2 113.2(2) . . ? C8 C7 H7A 108.9 . . ? N2 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? N2 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? O9 C8 C7 109.9(2) . . ? O9 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? O9 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? N2 C9 C10 110.2(2) . . ? N2 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? N2 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? O6 C10 O7 124.6(3) . . ? O6 C10 C9 119.1(3) . . ? O7 C10 C9 116.2(2) . . ? N2 C11 C12 110.0(2) . . ? N2 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O5 C12 C11 108.7(2) . . ? O5 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? O5 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.3 . . ? N3 C13 C14 108.90(19) . . ? N3 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? N3 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? O12 C14 O11 124.4(2) . . ? O12 C14 C13 119.7(2) . . ? O11 C14 C13 115.9(2) . . ? N3 C15 C16 111.12(19) . . ? N3 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N3 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? O10 C16 C15 108.76(19) . . ? O10 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? O10 C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? N3 C17 C18 109.71(19) . . ? N3 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? N3 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? O8 C18 C17 107.90(18) . . ? O8 C18 H18A 110.1 . . ? C17 C18 H18A 110.1 . . ? O8 C18 H18B 110.1 . . ? C17 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.941 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.067